A production apparatus for a triazinone

Abstract

The utility model discloses a production device of triazinone belongs to triazinone production technical field, including the separation tank, the separation tank top is connected with hydrolytic kettle, acid supply jar and alkali supply jar respectively, be equipped with stirring subassembly on the separation tank, the separation tank lower end side wall is equipped with the liquid outlet, be equipped with filter screen on the liquid outlet, the liquid outlet is connected with waste liquid jar through the liquid outlet pipeline, along liquid flow direction, first liquid pump, first three -way valve are equipped with in proper order on the liquid outlet pipeline, one port of first three -way valve is connected with oxidation kettle through the liquid distribution pipeline, the oxidation kettle is connected with cyclization kettle, the utility model adds the separation tank between hydrolytic kettle and oxidation kettle, keeps oil phase and oil -water mixture in the separation tank, utilizes solubility and separates the material of separation tank with oil phase, and material is discharged into oxidation kettle and reacts, shortens production time, reduces material waste and equipment floor area.

Description

Technical Field

[0001] This utility model relates to the field of triazine ketone production technology, specifically to a triazine ketone production apparatus. Background Technology

[0002] Triazinones are a class of heterocyclic compounds with potential biological activity. Triazinones are essential raw materials for the synthesis of triazine, and their production mainly includes three stages: hydrolysis, oxidation, and cyclization. Current technologies mostly use dichloropinazone as a raw material for synthesis. Dichloropinazone reacts with liquid alkali to hydrolyze and generate a hydrolysate containing sodium 2-hydroxy-3,3-dimethylbutyrate. During hydrolysis, a small amount of light component oil layer is present. An increased amount of oil layer in the hydrolysate can adversely affect the subsequent oxidation reaction and may even poison the catalyst in the oxidation process.

[0003] When separating the oil layer by liquid-liquid separation, an intermediate layer of oil and water may easily exist. In the existing technology, multiple two-phase separation tanks are usually set up to separate the hydrolysate multiple times to remove the oil layer in the hydrolysate. However, the hydrolysate undergoes multiple oil-water phase separations in multiple two-phase separation tanks, which leads to a longer process time, increased material loss, and a large equipment footprint, which is not conducive to the long-term production of triazine ketone.

[0004] In view of the problems existing in the prior art, this utility model combines years of design and use experience in related fields to design and manufacture a triazine ketone production device to overcome the above defects. Summary of the Invention

[0005] To address the problems existing in the prior art, this utility model provides a triazine ketone production device that, by adding a separation tank, precipitates out the material in the small amount of hydrolysate that has not been separated from the oil phase, achieving complete separation from the oil phase without material loss, and reducing the equipment involved in production.

[0006] To achieve the above objectives, the technical solution adopted by this utility model is as follows: A triazine ketone production device includes a separation tank, a hydrolysis vessel, an acid supply tank, and an alkali supply tank connected to the top of the separation tank respectively. The separation tank is equipped with a stirring assembly, and a liquid outlet is provided on the lower side wall of the separation tank. A filter screen is provided on the liquid outlet. The liquid outlet is connected to a waste liquid tank through a liquid outlet pipe. Along the liquid flow direction, a first liquid pump and a first three-way valve are sequentially provided on the liquid outlet pipe. One port of the first three-way valve is connected to an oxidation vessel through a liquid distribution pipe. The oxidation vessel is connected to a cyclization vessel.

[0007] Preferably, the stirring assembly includes a motor located at the top of the separation tank. The output end of the motor is connected to a rotating rod, which is vertically arranged. The lower end of the rotating rod passes through the top of the separation tank and extends downward. The rotating rod is provided with a plurality of stirring rods.

[0008] Preferably, the lower end of the rotating rod is provided with a plurality of scrapers, the bottom end of the scrapers is in contact with the bottom surface of the inner wall of the separation tank, and the end of the scraper near the side wall of the separation tank is in contact with the filter screen.

[0009] Preferably, the bottom of the separation tank is provided with a slag discharge port, the slag discharge port is provided with a slag discharge pipe, and the slag discharge pipe is provided with a slag discharge valve.

[0010] Preferably, the separation tank is connected to the acid supply tank via a first pipe, and the first pipe is equipped with an acid valve.

[0011] Preferably, the separation tank is connected to the alkali supply tank via a second pipe.

[0012] Preferably, the second pipeline is provided with a second three-way valve, and one port of the second three-way valve is connected to a water supply tank through a third pipeline.

[0013] Preferably, two support rods are vertically provided at the top of the inner wall of the separation tank, and an annular tube is provided between the two support rods. The annular tube is located above the stirring rod and is coaxially arranged with the rotating rod. A plurality of nozzles are evenly distributed along the circumference of the annular tube. The annular tube is connected to the second pipeline.

[0014] Preferably, the alkali supply tank contains sodium hydroxide solution, and the acid supply tank contains hydrochloric acid.

[0015] The advantages of this utility model are:

[0016] 1. This utility model adds a separation tank between the hydrolysis tank and the oxidation tank. After preliminary oil-water separation in the separation tank, the aqueous layer enters the oxidation tank for further reaction, while the upper oil phase and a small amount of unseparated intermediate layer are retained. Utilizing the difference in solubility, the acid supply tank converts sodium 2-hydroxy-3,3-dimethylbutyrate into 2-hydroxy-3,3-dimethylbutyric acid, which precipitates from the aqueous phase, thus completely separating the material from the oil phase. Then, the alkali supply tank converts 2-hydroxy-3,3-dimethylbutyric acid back into sodium 2-hydroxy-3,3-dimethylbutyrate and redissolves it in water, thereby reducing material loss. A filter screen is installed to prevent 2-hydroxy-3,3-dimethylbutyric acid from being discharged with the liquid.

[0017] 2. This utility model is designed so that the scraper contacts the filter screen and the bottom surface of the inner wall of the separation tank, stirring up the material at the bottom, accelerating the reaction, and preventing impurities from clogging the filter screen; it is also designed so that the scraper can scrape impurities into the slag discharge port for easy cleaning. Attached Figure Description

[0018] Figure 1 This is a schematic diagram of a triazine ketone production apparatus.

[0019] In the diagram: 1-Hydrolysis reactor, 2-Separation tank, 3-Oxidation reactor, 4-Circulation reactor, 5-Acid supply tank, 6-First pipeline, 7-Acid valve, 8-Waste liquid tank, 9-Discharge pipeline, 10-First pump, 11-First three-way valve, 12-Separation pipeline, 13-Alkali supply tank, 14-Second pipeline, 15-Second three-way valve, 16-Third pipeline, 17-Hydrolysis valve, 18-Second pump, 19-Fourth pipeline, 20-Third pump, 21-Oxidation valve, 22-Filter screen, 23-Motor, 24-Rotating rod, 25-Stirring rod, 26-Scraper, 27-Slag discharge port, 28-Slag discharge pipeline, 29-Slag discharge valve, 30-Support rod, 31-Ring pipe, 32-Nozzle, 33-Fifth pipeline, 34-Water supply tank. Detailed Implementation

[0020] To facilitate understanding by those skilled in the art, the present invention will be further described below with reference to the accompanying drawings.

[0021] like Figure 1 As shown, a triazine ketone production apparatus includes a separation tank 2, with a hydrolysis vessel 1, an acid supply tank 5, and an alkali supply tank 13 connected to the top of the separation tank 2. A liquid outlet is provided on the lower side wall of the separation tank 2, and a filter screen 22 is installed on the outlet. The outlet is connected to a waste liquid tank 8 via an outlet pipe 9. Along the liquid flow direction, a first pump 10 and a first three-way valve 11 are sequentially installed on the outlet pipe 9. One port of the first three-way valve 11 is connected to an oxidation vessel 3 via a separating pipe 12. The oxidation vessel 3 is connected to a cyclization vessel 4. The hydrolysis vessel 1, oxidation vessel 3, and cyclization vessel 4 are all conventional devices in the art. The hydrolysate undergoes an oxidation reaction with a sodium hypochlorite solution in the oxidation vessel 3, and then the oxidized solution enters the cyclization vessel 4 to undergo a cyclization reaction with thiocarbazone to obtain triazine ketone.

[0022] This invention adds a separation tank 2 between the hydrolysis reactor 1 and the oxidation reactor 3. The hydrolysate first enters the separation tank 2 to settle and separate into layers. The lower layer of hydrolysate enters the oxidation reactor 3, while the upper oil phase and the intermediate layer are retained. Utilizing the difference in solubility, acid is introduced through the acid supply tank 5 to convert the small amount of sodium 2-hydroxy-3,3-dimethylbutyrate contained in the intermediate layer into 2-hydroxy-3,3-dimethylbutyric acid, which then precipitates. The resulting waste liquid enters the waste liquid tank 8, where it separates into layers and undergoes waste treatment. The waste treatment is a conventional method and will not be described in detail here. Then, alkali is added through the alkali supply tank 13 to convert the 2-hydroxy-3,3-dimethylbutyric acid into a sodium salt that dissolves in the aqueous phase. This reduces material loss during complete separation of the oil phase, shortens the production time of triazine ketone, and reduces the equipment footprint. The filter screen 22 prevents 2-hydroxy-3,3-dimethylbutyric acid from being discharged with the waste liquid.

[0023] Specifically, the separation tank 2 and the acid supply tank 5 are connected via a first pipe 6, which is equipped with an acid valve 7. The separation tank 2 is connected to the alkali supply tank 13 via a second pipe 14, which is equipped with a second three-way valve 15. One port of the second three-way valve 15 is connected to a water supply tank 34 via a third pipe 16. The water supply tank 34 adds deionized water to the separation tank 2 to wash away the precipitated 2-hydroxy-3,3-dimethylbutyric acid and remove the oil layer adhering to its surface. The separation tank 2 and the hydrolysis vessel 1 are connected via a fourth pipe 19, which is equipped with a second liquid pump 18 and a hydrolysis valve 17. The oxidation vessel 3 and the cyclization vessel 4 are connected via a fifth pipe 33, which is equipped with a third liquid pump 20 and an oxidation valve 21. The acid supply tank 5 contains hydrochloric acid, and the alkali supply tank 13 contains sodium hydroxide solution. Hydrochloric acid and sodium hydroxide are selected as reagents to avoid introducing impurity ions into the waste liquid and hydrolysate.

[0024] The separator 2 is equipped with a stirring assembly, which includes a motor 23 located at the top of the separator 2. The output end of the motor 23 is connected to a rotating rod 24, which is vertically positioned and extends downwards through the top of the separator 2. Several stirring rods 25 are mounted on the rotating rod 24 and are located inside the separator 2. The stirring rods 25 agitate the liquid, accelerating the reaction. Several scrapers 26 are located at the lower end of the rotating rod 24, with their bottom ends contacting the bottom surface of the inner wall of the separator 2. These scrapers stir up the material at the bottom, preventing material accumulation and extending the reaction time. One end of the scraper 26 near the inner wall of the separator 2 contacts the filter screen 22, preventing clogging. A slag discharge port 27 is located at the bottom of the separator 2, with a slag discharge pipe 28 and a slag discharge valve 29. The scrapers 26 scrape impurities from the hydrolysate into the slag discharge port 27 for easy cleaning. An impurity trough is located below the slag discharge pipe 28 for collecting impurities.

[0025] Two support rods 30 are vertically installed at the top of the inner wall of the separator 2, and an annular tube 31 is provided between the two support rods 30. The support rods 30 are used to support the annular tube 31. The annular tube 31 is located above the stirring rod 25 and is coaxially arranged with the rotating rod 24. Several nozzles 32 are evenly distributed along the circumference of the annular tube 31; the annular tube 31 is connected to the second pipe 14. Sodium hydroxide solution and deionized water are evenly sprayed into the separator 2 through the nozzles 32.

[0026] Detailed operation process

[0027] After the hydrolysis of dichloropinazone and liquid alkali is completed in hydrolysis reactor 1, the second pump 18 and hydrolysis valve 17 are opened to pump the hydrolysate from hydrolysis reactor 1 into separation tank 2. After standing for a period of time, the liquid separates into layers in separation tank 2: the upper layer is the oil phase, the middle layer is the oil-water mixture, and the lower layer is the aqueous phase. The connection between separation tank 2 and oxidation reactor 3 is opened by opening the first three-way valve 11, and the first pump 10 is opened, allowing the lower aqueous phase to enter oxidation reactor 3. The oil phase and oil-water mixture are retained in separation tank 2. The connection between separation tank 2 and oxidation reactor 3 is then closed by closing the first three-way valve 11.

[0028] Start motor 23, which drives rotating rod 24 to rotate. Rotating rod 24 drives stirring rod 25 and scraper 26 to rotate, stirring the liquid. Open acid valve 7 on first pipe 6 to add hydrochloric acid from acid supply tank 5 to separation tank 2. Sodium 2-hydroxy-3,3-dimethylbutyrate in the oil-water mixture is converted to 2-hydroxy-3,3-dimethylbutyric acid under acidic conditions and precipitates from the liquid. After the solid has completely precipitated, open the connection between separation tank 2 and waste liquid tank 8 on first three-way valve 11, turn on first pump 10 to discharge liquid from separation tank 2 into waste liquid tank 8, and close the connection between separation tank 2 and waste liquid tank 8 on first three-way valve 11. Then open the connection between water supply tank 34 and separation tank 2 on second pipe 14, second three-way valve 15. Deionized water enters annular pipe 31 from third pipe 16 and is sprayed out from nozzle 32. Deionized water is used to wash the solid, removing the oil layer adhering to the solid surface.

[0029] After washing, close the connection between the water supply tank 34 and the separation tank 2 on the second three-way valve 15, open the connection between the separation tank 2 and the waste liquid tank 8 on the first three-way valve 11, and turn on the first liquid pump 10 to discharge the liquid in the separation tank 2 into the waste liquid tank 8. Then close the connection between the separation tank 2 and the waste liquid tank 8 on the first three-way valve 11. Open the connection between the alkali supply tank 13 and the separation tank 2 on the second three-way valve 15, and add the sodium hydroxide solution from the alkali supply tank 13 into the separation tank 2 through the nozzle 32. 2-Hydroxy-3,3-dimethylbutyric acid is converted into sodium salt and dissolved in the solution. Then close the connection between the alkali supply tank 13 and the separation tank 2 on the second three-way valve 15. Open the connection between the separation tank 2 and the oxidation vessel 3 on the first three-way valve 11, and turn on the first liquid pump 10. The liquid enters the oxidation vessel 3. The hydrolysate is oxidized in the oxidation vessel 3 to obtain keto acids, which then enter the cyclization vessel 4 for a cyclization reaction to obtain triazine ketones.

[0030] It should be understood that these embodiments are for illustrative purposes only and are not intended to limit the scope of protection of this utility model. Furthermore, it should be understood that after reading the technical description of this utility model, those skilled in the art can make various alterations, modifications, and / or variations to this utility model, and all such equivalent forms also fall within the scope of protection defined by the appended claims.

Claims

1. A production apparatus for triazine ketone, characterized in that, The system includes a separation tank (2), on the top of which are connected a hydrolysis vessel (1), an acid supply tank (5), and an alkali supply tank (13). The separation tank (2) is equipped with a stirring assembly, and the lower side wall of the separation tank (2) is provided with a liquid outlet. A filter screen (22) is provided on the liquid outlet. The liquid outlet is connected to a waste liquid tank (8) through a liquid outlet pipe (9). Along the liquid flow direction, a first liquid pump (10) and a first three-way valve (11) are sequentially provided on the liquid outlet pipe (9). One port of the first three-way valve (11) is connected to an oxidation vessel (3) through a liquid distribution pipe (12). The oxidation vessel (3) is connected to a cyclization vessel (4).

2. The triazine ketone production apparatus according to claim 1, characterized in that, The stirring assembly includes a motor (23), which is located at the top of the separation tank (2). The output end of the motor (23) is connected to a rotating rod (24). The rotating rod (24) is vertically arranged, and the lower end of the rotating rod (24) passes through the top of the separation tank (2) and extends downward. Several stirring rods (25) are provided on the rotating rod (24).

3. The triazine ketone production apparatus according to claim 2, characterized in that, The lower end of the rotating rod (24) is provided with several scrapers (26). The bottom end of the scraper (26) is in contact with the bottom surface of the inner wall of the separation tank (2). The end of the scraper (26) near the side wall of the separation tank (2) is in contact with the filter screen (22).

4. The triazine ketone production apparatus according to claim 1, characterized in that, The bottom of the separation tank (2) is provided with a slag discharge port (27), the slag discharge port (27) is provided with a slag discharge pipe (28), and the slag discharge pipe (28) is provided with a slag discharge valve (29).

5. The triazine ketone production apparatus according to claim 1, characterized in that, The separation tank (2) is connected to the acid supply tank (5) through a first pipe (6), and an acid valve (7) is provided on the first pipe (6).

6. The triazine ketone production apparatus according to claim 2, characterized in that, The separation tank (2) is connected to the alkali supply tank (13) via a second pipe (14).

7. The triazine ketone production apparatus according to claim 6, characterized in that, The second pipe (14) is equipped with a second three-way valve (15), and one port of the second three-way valve (15) is connected to a water supply tank (34) through a third pipe (16).

8. The triazine ketone production apparatus according to claim 6, characterized in that, The inner wall of the separation tank (2) is vertically provided with two support rods (30), and an annular tube (31) is provided between the two support rods (30). The annular tube (31) is located above the stirring rod (25) and is coaxially arranged with the rotating rod (24). Several nozzles (32) are evenly distributed along the circumference of the annular tube (31). The annular tube (31) is connected to the second pipe (14).

9. A triazine ketone production apparatus according to claim 1, characterized in that, The alkali supply tank (13) contains sodium hydroxide solution, and the acid supply tank (5) contains hydrochloric acid.

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